Reactions with concentrated

Reaction with chlorosulphonic acid ( chlorosulphonyl-ation ). Sulphonamides. Many aryl hahdes, either alone or in chloroform solution, when treated with excess of chlorosulphonic acid afford the corresponding sulphonyl chlorides in good yield (compare Section IV.106) the latter may be readily converted into the aryl sulphonamides by reaction with concentrated ammonia solution or with sohd ammonium carbonate. 

Sodium reacts with dilute acids about as vigorously as it reacts with water. The reaction with concentrated sulfuric acid may be somewhat less vigorous. At 300—385°C, sodium and sodium hydroxide react according to the following equiUbrium ... 

The calcium chloride content of Ca(OCl)2 slurries or filter cakes can be reduced or eliminated by reaction with concentrated, low salt NaOCl solution (181). 

Nitrates have only been prepared from saturated equatorial 3-hydroxyl groups by reaction with concentrated nitric acid and acetic anhydride at low temperature.Electrophilic substitution at C-6 precludes the satisfactory formation of nitrates from A -3j5-ols. 

In contrast to other acids, anhydrous hydrogen fluoride does not cause hydroly SIS and decarboxylation of the malonic acid residues in these reactions [5]. It is a good reagent for the cyclization of a-benzamidoacetophenones to 2,5 diphenyl-oxazoles [6] (equation 7) The same reaction with concentrated sulfuric acid gives cyclic product with only a 12% yield [6]... 

Reaction with concentrated acids provides a preparative route to nitrosyl salts such as N0[HS04], N0[HSe04], N0[C104], and NO[Bp4], e.g. ... 

This technique for catalyst regeneration has recently been utilized with great success in ATRA reactions catalyzed by [Cp Ru"lCI/PPh ) [169,170] and [Cun(TPMA)X][X] [118,119] (X = Br and Cl ) complexes. The activity of [Cun(TPMA)Br][Br] complex in ATRA of polybrominated compounds to alkenes in the presence of AIBN, based on catalyst loading, conversion of alkene, and the yield of monoadduct, was approximately ten times higher than the activity of [Cun(TPMA)Cl][Cl], This complex, in conjunction with AIBN, effectively catalyzed ATRA reactions with concentrations between 5 and 100 ppm, which was by far the lowest number achieved in copper-mediated ATRA. 

HD on laboratory glassware may be oxidized by its vigorous reaction with concentrated nitric acid. 

Note Surfaces contaminated with T, then rinse-decontaminated may evolve sufficient T vapor to produce a physiological response. T on laboratory glassware may be oxidized by it vigorous reaction with concentrated nitric acid. 

Thiocarbonyl compounds are converted into the corresponding carbonyl derivatives in good yield (70-99%) by their reaction with concentrated aqueous sodium hydroxide and dichloromethane in the presence of tetra-n-butyiammonium hydrogen sulphate [4], The reaction is general for thioeslers, thioamides, thioureas and thiones (Table 3.28), and no reaction occurs in the absence of the phase-transfer catalysts. The reaction is also aided by the initial 5-methylation of the thiocarbonyl group [5]. 

Air (NB) Collection in ethanol reaction with concentrated HCl and zinc dust react with sodium salt of 1,2-naphtho-quinone-4 sulfonic acid at pH 8.0 extraction with CCl concentration separation by paper chromatography extraction of fractions with CCl ... 

Ordinarily arsenic does not react with water, hydrogen, caustic soda or hydrochloric acid. However, in presence of an oxidant it reacts with concentrated HCl. In concentrated HCl solution it reacts with hydrogen sulfide to form a precipitate of yellow arsenic sulfide, AS2S3. It forms orthoarsenic acid, H3ASO4 on reaction with concentrated nitric acid and chlorinated water. 

Similarly, arsenic tribromide AsBrs forms when the trioxide reacts with bromine vapors. Reaction with concentrated HCI under heating produces arsenic trichloride. 

Reaction with concentrated sulfuric acid yields hydrogen fluoride and calcium sulfate ... 

Europeum generally is produced from two common rare earth minerals monazite, a rare earth-thorium orthophosphate, and bastnasite, a rare earth fluocarbonate. The ores are crushed and subjected to flotation. They are opened by sulfuric acid. Reaction with concentrated sulfuric acid at a temperature between 130 to 170°C converts thorium and the rare earths to their hydrous sulfates. The reaction is exothermic which raises the temperature to 250°C. The product sulfates are treated with cold water which dissolves the thorium and rare earth sulfates. The solution is then treated with sodium sulfate which precipitates rare earth elements by forming rare earth-sodium double salts. The precipitate is heated with sodium hydroxide to obtain rare earth hydrated oxides. Upon heating and drying, cerium hydrated oxide oxidizes to tetravalent ceric(lV) hydroxide. When the hydrated oxides are treated with hydrochloric acid or nitric acid, aU but Ce4+ salt dissolves in the acid. The insoluble Ce4+ salt is removed. 

Reaction with concentrated hydrochloric acid yields gold(lII) chloride ... 

While treatment with aqueous sulfuric acid hydrolyzes hydrogen cyanide to formic acid, HCOOH, its reaction with concentrated sulfuric acid is violent forming an adduct HCN H2S04. The adduct is unstable, decomposing to carbon dioxide, sulfur dioxide and ammonia ... 

Reaction with concentrated acetic acid yields anhydrous leadfll) acetate. 

Reactions with concentrated acids are slow at room temperature, but rapid when heated. No hydrogen forms in concentrated acids. With concentrated sulfuric and nitric acids, sulfur dioxide and nitric oxide form ... 

Technetium dissolves in dilute or concentrated nitric acid to form nitrate, Tc(N03)2. Reaction with concentrated sulfuric acid yields the sulfate TCSO4. Technetium is oxidized by hydrogen peroxide in alkaline solution to form soluble pertechnetate, Tc04 anion. Such pertechnatate anion forms complexes with tertiary or quarternary amines, pyridine and its methyl-substituted derivatives. 

The physical properties of the metal (Table II) resemble those of thallium, lead and bismuth, its neighbors in the Periodic Table, rather than those of tellurium, its lower homologue. The low melting and boiling points are particularly noteworthy an attempted study of the Hall effect in polonium metal has also been reported (90). In chemical properties the metal is very similar to tellurium, the most striking resemblance being in its reactions with concentrated sulfuric acid (or sulfur trioxide) and with concentrated selenic acid. The products are the bright red solids, PoSOs and... 

Secondary and tertiary propargyl alcohols are directly converted to halo-allenes on reaction with concentrated aqueous hydrogen halides in the presence of the corresponding cuprous halide [60,72-73]. (See Table VII.) Better yields are obtained with hydrogen bromide. Hydrogen chloride yields chloroallene, propargyl chloride, and the chloro- 1,3-diene isomers (Eq. 60). 

Ethylene sulfide,8 propylene sulfide,88 3-ohloropropylene sulfide,18 and cyclohexene sulfide1 have been converted into 2-chlarothioIs in 33, 60, 72, end 67% yields respectively by reaction with concentrated hydrochloric add. Dilute hydrochloric add, however, leads to more extensive polymerization. 3ft... 

Bromo-l,l,2-trifluoroethyl methyl ether on reaction with concentrated sulfuric acid gives methyl bromofluoroacetate (27).149... 

There is surprisingly little reliable information on the sulfonation of benzo[6]thiophene or its derivatives. Benzo[6]thiophene is more readily sulfonated than naphthalene.699 Reaction with concentrated sulfuric acid at 80° gives a mixture of mono-, di-, and trisulfonic acids, reaction with 70% sulfuric acid at 80° gives a monosulfonic acid,699 and reaction with 18% oleum gives a disulfonic acid 86 in each case the orientation of the products is unknown. Treatment of benzo[6]thiophene with concentrated sulfuric acid in acetic anhydride at 20° gives 3-acetylbenzo[6]thiophene (ca. 10%) and a sulfonation product (isolated as the potassium salt), which was believed to be the 3-sulfonic acid.660 Recently, the sulfonation product has been shown to contain the 2- (8%) and 3-isomer (92%), by conversion into the sulfonyl chlorides and reduction to a separable mixture of 2- and 3-mercaptobenzo[6]thiophene.84... 

Sodium perchlorate (NaC104) is produced commercially by the electrolytic oxidation of aqueous sodium chlorate and is converted to perchloric acid by reaction with concentrated HC1 ... 

As a consequence, there is a very significant energy barrier towards removal of the metal from the complex, although prolonged reaction with concentrated cyanide is sometimes successful. This kinetic stability of the complex leads to some remarkable properties... 

Cadmium Phosphide Cd3P2 Nitric Acid. Reaction with concentrated acid is explosive.9... 

Ammonia. Violent reaction with concentrated aqueous ammonia.3,4 Tertiary Bases. In absence of solvent, reaction may be explosive.5... 

Nitric Acid. Explosive reaction with concentrated acid.30... 

Cyclopentadiene. Violent or explosive reaction with concentrated acid.11... 

Sodium. Slow reaction with anhydrous acid explosive reaction with aqueous acid.28 Sodium Borohydride. Reaction with concentrated sulfuric acid to yield diborane may... 

We discussed making 57 from the lactone 59 in chapter 25 and we have used the ketoester 60 in chapters 19 and 25. Alkylation of 60 gives 61, reaction with concentrated HC1 gives the acid corresponding to 55 and polyphosphoric acid (PPA) catalyses the cyclisation to 54. 

A mixture of 61 grams l-phenyl-l-oxo-2-(N-methyl-N-ethanolamino)-propane hydrochloride and 100 cc 98-100% formic acid was refluxed at the boiling point at atmospheric pressure for 45 minutes on an oil bath. Thereafter, the oil bath temperature was increased to 180°C and as much of the excess unreacted formic acid as possible was distilled off. A vigorous evolution of carbon dioxide developed during the distillation, which ceased after approximately 45 additional minutes. The honey-yellow syrup which remained as the distillation residue was worked up by admixing it with about six volumes of water and adjusting the aqueous mixture to alkaline reaction with concentrated sodium hydroxide. An oily phase separated out which was extracted with ether. The ether extract was washed with water and dried over potassium carbonate. The solvent was distilled off and the distillation residue was fractionally distilled in vacuo. The base boils at 132°-133°C at 12 mm. The yield was 93% of theory. Reaction with tartaric acid gave the final product. 

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